HRID1105886

反应详情

EQUATION

反应方程式

HRID 1105886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

45 g of 1-(2,4,6-trichlorophenyl)-3-{3-[2-(2,4-di-tert-amylphenoxy)butyramido]benzamido}-4-bromo-5-oxo-2-pyrazoline and 19 g of 4-methylpyrazole were mixed with each other, then stirred for 2 hours under heating at 90° C. To the reaction mixture was added 500 ml of ethyl acetate, followed by washing several times with water. The ethyl acetate layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from a solvent mixture of 100 ml of acetonitrile and 20 ml of benzene, 19 g of Coupler (2) was obtained. The melting point of the coupler was 142° to 145° C.

WORKUP

后处理

  1. washby washing several times with water
  2. dry with materialThe ethyl acetate layer was dried with anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customUpon crystallization of the residue
  5. additionfrom a solvent mixture of 100 ml of acetonitrile and 20 ml of benzene, 19 g of Coupler (2)
  6. customwas obtained
  7. customwas 142° to 145° C.